CN1240670C - Process of separating DL-alpha lactamic acid by ion membrane electric dialysis method - Google Patents
Process of separating DL-alpha lactamic acid by ion membrane electric dialysis method Download PDFInfo
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- CN1240670C CN1240670C CN 200410016417 CN200410016417A CN1240670C CN 1240670 C CN1240670 C CN 1240670C CN 200410016417 CN200410016417 CN 200410016417 CN 200410016417 A CN200410016417 A CN 200410016417A CN 1240670 C CN1240670 C CN 1240670C
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- bing ansuan
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Abstract
The present invention relates to a technology for separating DL-alpha-alanine by an ion membrane electrodialysis method, which is characterized in that synthetic mixed liquid of DL-alpha-alanine and ammonium chloride is introduced in an ion membrane electrodialyzer; ion membrane electrodialysis is formed by cation exchange membranes and anion exchange membranes by different arrangement sequence; under the action of a direct current electric field, NH4<+> migrates towards a cathode direction through the cation exchange membranes, and Cl<-> migrates towards an anode direction through the anion exchange membranes; after cycling separation, a DL-alpha-alanine solution and an ammonium chloride solution can be respectively acquired; products of the DL-alpha-alanine and the ammonium chloride are crystallized and separated out. The method has the advantages of obvious reduction of energy source consumption, no need of the adoption of a large quality of combustible toxic methanol, low production cost, basic removal of three wastes, improvement of the product quality and acquirement of high-quality ammonium chloride as by-products.
Description
Technical field
The present invention separates DL-α-Bing Ansuan novel process for a kind of in preparation DL-α-Bing Ansuans such as utilizing the α-Lv Bingsuan ammoniation process is produced, its characteristics are to use cationic exchange membrane and anion-exchange membrane, arrange by different order, form ionic membrane electrodialysis tripping device, DL-α-Bing Ansuan and ammonium chloride mixed solution are carried out membrane sepn, relate to technology and operating parameters that the electrodialysis of utilization ionic membrane separates DL-α-Bing Ansuan and ammonium chloride.
Background technology
The DL-α-Bing Ansuan is a kind of important amino acid, be the important source material and the intermediate in fields such as medicine industry, agro-industry, organic synthesis and biochemical research, as foodstuff additive, fodder additives, daily use chemicals auxiliary agent etc., also be widely used in the industries such as food, feed, daily use chemicals.
Existing DL-α-Bing Ansuan is synthetic with separation method to be: with α-Lv Bingsuan, liquefied ammonia (or ammoniacal liquor) is raw material, is catalyzer with the urotropine, synthetic DL-α-Bing Ansuan and the ammonium chloride mixed solution of obtaining in the aqueous solution or alcohol solution or alcoholic solution; Utilize DL-α-Bing Ansuan undissolved characteristics in methyl alcohol, with a large amount of methyl alcohol the DL-α-Bing Ansuan separated to separate out, filter, make with extra care, drying obtains the DL-α-Bing Ansuan.Mother liquor is methyl alcohol and ammonium chloride mixt, reclaims methyl alcohol through rectifying, and the rectifying resistates obtains part through evaporation and is worth very low low-grade ammonium chloride, all the other dischargings.
The shortcoming that separating out alcohol method separates DL-α-Bing Ansuan technology is: 1, a large amount of mother liquors need rectifying to reclaim, and steam consumption is very big, and product per ton needs 9-12 ton steam.2, the methyl alcohol volatilization is big, consumes height, causes production cost to rise.3, use a large amount of inflammable virose methyl alcohol, cause production environment seriously polluted, also increased the production insecurity.4, ammonium chloride concentration height in the mother liquor, corrodibility is strong, rectifying tower requirement for anticorrosion height, investment is big, the maintenance cost height.5, separation yield is low.6, by-product ammonium chloride purity is low, is worth not high.
Summary of the invention
Purpose of the present invention is exactly at above-mentioned all kinds of shortcoming, adopt ionic membrane electroosmose process DL-α-Bing Ansuan and ammonium chloride mixed solution to carry out membrane sepn, have under the condition of normal temperature, no phase transformation realization separating substances and separation yield height, do not produce pollution characteristics.
Ionic membrane electroosmose process of the present invention separates DL-α-Bing Ansuan technology, it is characterized in that synthesizing the DL-α-Bing Ansuan and the ammonium chloride mixed solution that obtain introduces in the ionic membrane electrodialysis tripping device, utilization cationic exchange membrane and anion-exchange membrane, arrange by different order, form the ionic membrane electrodialysis under the DC electric field effect, NH
4Move to cathode direction by cationic exchange membrane, Cl is by the migration of anion-exchange membrane anode direction, and circulation can obtain DL-α-Bing Ansuan solution and ammonium chloride solution respectively after separating, and DL-α-Bing Ansuan and ammonium chloride product are separated out in crystallization.
The above-mentioned employing in the ionic membrane electrodialysis tripping device, its cationic exchange membrane and anionresin film put in order with difference, form multi-cavity chamber repeated arrangement, and the chamber number can be 2-5.
A kind of priority scheme of ionic membrane electrodialysis tripping device of the present invention is 2 chamber structures, be spaced by cationic exchange membrane and anion-exchange membrane, the chamber that the positive and negative ion-exchange membrane is formed is to mix liquid chamber, anion-exchange membrane is the salt chamber with organizing the cationic exchange membrane composition down, mix liquid chamber near negative electrode, the salt chamber is near anode, can carry out pH value to the DL-α-Bing Ansuan introduced and ammonium chloride mixed solution and be controlled at 5.5-6.5, prevent the partial ionization of DL-α-Bing Ansuan and move escape, see Fig. 1.Make when mixing liquid chamber ammonium chloride and reaching certain little concentration when the ionic membrane electrodialysis separates desalination, can obtain DL-α-Bing Ansuan solution and ammonium chloride solution respectively, separate out DL-α-Bing Ansuan and ammonium chloride product through condensing crystal.
The another kind of priority scheme of ionic membrane electrodialysis tripping device of the present invention is 3 chamber structures, by putting in order of cationic exchange membrane, cationic exchange membrane, anion-exchange membrane, the ionic membrane electrodialysis tripping device of forming 3 chamber repeated arrangement, the chamber that the positive and negative ion-exchange membrane is formed is amino acid feedback chamber, the chamber that the positive and negative ion-exchange membrane is formed is to mix liquid chamber, DL-α-Bing Ansuan and the ammonium chloride mixed solution introduced, anion-exchange membrane is the salt chamber with organizing the cationic exchange membrane composition down.Amino acid feedback chamber is near negative electrode, and the salt chamber is near anode.The DL-α-Bing Ansuan of introducing and the PH of ammonium chloride mixed solution are can be controlled in PH between 2-7, and preferred PH is between the 4.5-6; Amino acid feedback chamber PH can be controlled between the 5-8.5, and preferred PH is between the 6-7.The DL-α-Bing Ansuan has partial ionization in the mixing liquid chamber, and the DL-α-Bing Ansuan that ionization is moved out can enter into amino acid feedback chamber, can turn back to the mixing liquid chamber during to finite concentration, sees Fig. 2.Make when mixing liquid chamber ammonium chloride and reaching certain little concentration when the ionic membrane electrodialysis separates desalination, can obtain DL-α-Bing Ansuan solution and ammonium chloride solution respectively, separate out DL-α-Bing Ansuan and ammonium chloride product through condensing crystal.
Cationic exchange membrane and anion-exchange membrane that described ionic membrane electrodialysis tripping device is selected for use can be heterogeneous membrane or homogeneous membrane.The sum of separate unit electrodialysis tripping device intermediate ion exchange membrane can be in 1200, the size dimension of film is long 100mm-2000mm, wide 100mm-1200mm, the combination of separate unit ionic membrane electrodialysis tripping device can be one section one-level or one section multistage (secondary or more than the secondary), but serial or parallel connection between every grade.
Ionic membrane electroosmose process of the present invention separates DL-α-Bing Ansuan technology, and institute's ionic membrane electrodialysis tripping device that adopts is an ionic membrane electrodialysis tripping device, also available (contain two) more than two and carry out serial or parallel connection make up, with raising throughput.
The significant parameter that should control in operating process comprises current density, liquid flow velocity and temperature in each chamber, pH value.The current density increase helps improving the product segregation rate, but the selection of current density should be taken into account employed ion selective membrane ability to bear and limit current density, greater than limit current density the time, dissociating of water can be taken place, influence current efficiency, general current density should be at 1mA/cm
2-100mA/cm
2In the scope; Each chamber liquid circular flow increases and helps increasing the velocity of flow of liquid in chamber, reduce resistance to mass transfer and polarization phenomena, but liquid flow rate is excessive, easily makes between each chamber pressure equilibrium control improper, causes the pressure reduction infiltration.Therefore general controlled liq speed is in 0.1cm/s～100cm/s scope.Service temperature suitably raising helps accelerating ion migration speed, the ionic membrane electrodialysis process is accelerated, but the selection of service temperature should be considered the ability to bear of the film that uses, and general temperature should be between 5 ℃～100 ℃.
In the described circulating sepn process, the circulation fluid of each chamber is the aqueous solution or alcohol solution or alcoholic solution, and selected alcohol is methyl alcohol or ethanol or Virahol.
Advantage of the present invention:
First: avoided using a large amount of methyl alcohol and the serious methyl alcohol volatile emission that causes is polluted and the production insecurity.Second: the ionic membrane sepn process is no phase transition process, and is lower than the phase transition process power consumption, and ionic membrane electroosmose process separating technology reduces power consumption more than 50% than separating out alcohol method technology.The the 3rd: in the ionic membrane tripping device, except that small portions such as fastening piece are made of metal, being various macromolecular materials makes, these insulated with material and erosion resistance are all fine, there is not the such heavy corrosion problem of distillation method, the membrane separation unit long service life, operating maintenance is convenient, invest relatively for a short time, easily realize automatization control.The the 4th: the separation yield height.The 5th: by-product ammonium chloride purity is also high, and the added value height has reduced the three wastes.
Description of drawings
Fig. 1 is the structure iron of the ionic membrane electrodialysis tripping device of 2 chamber structures
Among the figure: CM is a cationic exchange membrane; AM is an anion-exchange membrane; R1 is for mixing liquid chamber; R2 is the salt chamber; RC is a cathode compartment; RA is the anolyte compartment; (+) is anode; (-) is negative electrode.
Fig. 2 is the structure iron of the ionic membrane electrodialysis tripping device of 3 chamber structures
Among the figure: CM is a cationic exchange membrane; AM is an anion-exchange membrane; R1 is for mixing liquid chamber; R2 is the salt chamber; R3 is amino acid feedback chamber; RC is a cathode compartment; RA is the anolyte compartment; (+) is anode; (-) is negative electrode.
Embodiment
Embodiment 1
Referring to Fig. 1, present embodiment is for adopting the ionic membrane electrodialysis tripping device of 2 chamber structures, and membrane area is 150mm * 300mm, 31 pairs of positive and negative ion-exchange membrane 2 chamber repeated arrangement.In operating process, the water mixed liquid of DL-α-Bing Ansuan and ammonium chloride is entered into electrodialysis tripping device chamber R1 after secondary filter, can carry out pH value to the DL-α-Bing Ansuan introduced and ammonium chloride mixed solution and be controlled at 6.The significant parameter current density 10mA/cm that in operating process, should control
2, liquid flow velocity is 3cm/s in each chamber, temperature is 30 ℃.When separating desalination, the ionic membrane electrodialysis makes when mixing liquid chamber ammonium chloride and reaching certain little concentration, can obtain DL-α-Bing Ansuan solution and ammonium chloride solution respectively, separate out DL-α-Bing Ansuan and ammonium chloride product through condensing crystal, DL-α-Bing Ansuan yield is 91.0%.
Embodiment 2
Referring to Fig. 2, adopt the ionic membrane electrodialysis tripping device of 3 chamber structures, the ion-exchange membrane size is 200mm * 400mm, 3 chamber structure repeated arrangement are 100 groups.In operating process, introduce DL-α-Bing Ansuan and ammonium chloride water mixed solution among the electrodialysis tripping device chamber R1, carry out circulation type membrane and separate, actuating current density control 15mA/cm
2, liquid flow velocity is 2.8cm/s in each chamber, temperature is 35 ℃; The DL-α-Bing Ansuan of introducing and the PH of ammonium chloride mixed solution are controlled between the 5-6; Amino acid feedback chamber PH is controlled between the 6-7.5, and the DL-α-Bing Ansuan that ionization is moved out can enter into amino acid feedback chamber, can turn back to the mixing liquid chamber during to finite concentration.Behind circulation membrane sepn 5.5h, obtain DL-α-Bing Ansuan solution and ammonium chloride solution, separate out DL-α-Bing Ansuan and ammonium chloride product through condensing crystal, DL-α-Bing Ansuan yield is 97.5%.
Claims (2)
1, a kind of ionic membrane electroosmose process separates DL-α-Bing Ansuan technology, synthetic DL-α-Bing Ansuan that obtains and ammonium chloride mixed solution are introduced in the ionic membrane electrodialysis tripping device, and under the DC electric field effect, NH
4 +Move Cl to cathode direction by cationic exchange membrane
-Move by anion-exchange membrane anode direction, through behind the circulation membrane sepn of certain hour, obtain DL-α-Bing Ansuan solution and ammonium chloride solution respectively, DL-α-Bing Ansuan and ammonium chloride product are separated out in crystallization, it is characterized in that: described ionic membrane electrodialysis tripping device, press cationic exchange membrane, cationic exchange membrane, putting in order of anion-exchange membrane, the ionic membrane electrodialysis tripping device of forming 3 chamber repeated arrangement, sun, the chamber that cationic exchange membrane is formed is amino acid feedback chamber, sun, the chamber that anion-exchange membrane is formed is to mix liquid chamber, anion-exchange membrane is the salt chamber with organizing the cationic exchange membrane composition down, amino acid feedback chamber is near negative electrode, and the salt chamber is near anode.
2, ionic membrane electroosmose process according to claim 1 separates DL-α-Bing Ansuan technology, it is characterized in that the DL-α-Bing Ansuan of described introducing and the mixing liquid chamber PH of ammonium chloride mixed solution are controlled at PH between 5-6; Between the amino acid feedback chamber PH control 6-7.5.
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| Application Number | Priority Date | Filing Date | Title |
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| CN 200410016417 CN1240670C (en) | 2004-02-16 | 2004-02-16 | Process of separating DL-alpha lactamic acid by ion membrane electric dialysis method |
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| CN 200410016417 CN1240670C (en) | 2004-02-16 | 2004-02-16 | Process of separating DL-alpha lactamic acid by ion membrane electric dialysis method |
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| CN1240670C true CN1240670C (en) | 2006-02-08 |
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101851016B (en) * | 2010-07-07 | 2011-11-09 | 浙江华友钴业股份有限公司 | Method for processing ammonium chloride waste water |
| CN106349131B (en) * | 2016-08-26 | 2018-04-20 | 宁夏紫光天化蛋氨酸有限责任公司 | A kind of isolation and purification method of methionine |
| CN110372496A (en) * | 2019-08-30 | 2019-10-25 | 河南师范大学 | A kind of method of electrodialysis purification neopentyl glycol sodium formate mixed liquor |
| CN110746019A (en) * | 2019-09-27 | 2020-02-04 | 杭州蓝然环境技术股份有限公司 | Method for extracting free L-lysine in ammonia water eluent by membrane method |
| CN113663518B (en) * | 2021-07-30 | 2022-10-28 | 中国科学技术大学 | Ion cooperative distillation system for fine screening of special mixed ions and application thereof |
| CN113663517B (en) * | 2021-07-30 | 2022-10-28 | 中国科学技术大学 | Anion rectification system for fine screening of special anions and application thereof |
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